CN113091939A - Preparation method of high-sensitivity temperature sensor based on graphene/barium strontium titanate heterojunction - Google Patents
Preparation method of high-sensitivity temperature sensor based on graphene/barium strontium titanate heterojunction Download PDFInfo
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- CN113091939A CN113091939A CN202110333309.2A CN202110333309A CN113091939A CN 113091939 A CN113091939 A CN 113091939A CN 202110333309 A CN202110333309 A CN 202110333309A CN 113091939 A CN113091939 A CN 113091939A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/16—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements
- G01K7/22—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements the element being a non-linear resistance, e.g. thermistor
Abstract
The invention discloses a preparation method of a high-sensitivity temperature sensor based on a graphene/barium strontium titanate heterojunction, belongs to the field of temperature sensors, and aims to solve the problems of low sensitivity and response speed of the conventional temperature sensor. The preparation method comprises the following steps: firstly, preparing barium strontium titanate ceramic by adopting a solid-phase sintering method; secondly, cutting the graphene loaded on the copper sheet, and spin-coating polymethyl methacrylate on the graphene; thirdly, putting the graphene subjected to spin coating into a copper etching solution, and fishing the graphene from the copper etching solution; fourthly, transferring the graphene onto a polished surface of barium strontium titanate ceramic, and drying; fifthly, putting the dried barium strontium titanate ceramic into acetone to dissolve polymethyl methacrylate; sixthly, placing the graphene-barium strontium titanate heterojunction into an oven for drying. When the temperature rises to the vicinity of the phase transition temperature of barium strontium titanate, the respective rising rates of the currents are higher compared with the room temperature, and the current change rate is very high in a narrow phase transition temperature region, so that the detection sensitivity is higher.
Description
Technical Field
The invention belongs to the field of temperature sensors, and particularly relates to a preparation method of a graphene/barium strontium titanate heterostructure temperature sensor with high sensitivity.
Background
A temperature sensor is a device capable of converting a temperature signal into an electric signal and outputting the same, wherein the conversion into a resistance signal is the most common and easily designed method, and devices commonly used for measuring temperature include a thermocouple and a thermistor, wherein the thermistor related to a semiconductor is a principle of converting an increase signal of temperature into a decrease signal of resistance. Although thermistors are widely studied in the field of temperature sensors, many critical problems still need to be solved in terms of the critical materials and device structures of temperature sensors for which high sensitivity and high response speed are required, for example, the problem that high current causes self-heating of thermistors is still to be solved, and therefore, the search for novel high-sensitivity and high-response-speed temperature sensor materials and device structures is still a new challenge.
The appearance of the graphene opens a new research idea for the research of high-speed response devices. The ideal single layer graphene has a fully symmetric conical band structure. Bonds in the molecular structure are mutually conjugated to form large pi bonds, so that carriers can move at high speed, and the theoretical carrier mobility is about 200000cm2Vs, far exceeding that of indium antimonide (about 77000 cm) which has been considered to have the highest carrier mobility2Vs). However, the type of substrate may affect the carrier mobility of graphene. Specifically, the self-polarizing electric field of the ferroelectric dipole in the ferroelectric material has a significant effect on the graphene carrier properties and resistivity in the graphene/ferroelectric thin film heterostructure. These ferroelectric dipoles will disappear during the phase transition, and the Curie temperature can be used such as BaTiO3、PbZrTiO3And (K, Na) NbO3And adjusting the ion doping by using the dopant.
Disclosure of Invention
The invention aims to solve the problems of low sensitivity and response speed of the conventional temperature sensor, and provides a preparation method of a high-sensitivity temperature sensor based on a graphene/barium strontium titanate heterojunction.
The preparation method of the high-sensitivity temperature sensor based on the graphene/barium strontium titanate heterojunction is realized according to the following steps:
firstly, adopting a solid-phase sintering method according to BaxSr1-xTiO3Preparing barium strontium titanate ceramic according to the stoichiometric ratio and polishing;
secondly, cutting the graphene loaded on the copper sheet, and spin-coating a layer of polymethyl methacrylate on the graphene to obtain the spin-coated graphene;
thirdly, putting the spin-coated graphene into a copper etching solution, fishing out the graphene from the copper etching solution, and putting the graphene into deionized water for cleaning to obtain clean graphene;
transferring the cleaned graphene to a polished surface of the barium strontium titanate ceramic by adopting a wet transfer method, and then putting the barium strontium titanate ceramic into an oven for drying to obtain dried barium strontium titanate ceramic;
fifthly, putting the dried barium strontium titanate ceramic into acetone to dissolve polymethyl methacrylate on the surface of the graphene, and then putting the graphene into deionized water to clean the graphene and the barium strontium titanate heterojunction to obtain the graphene-barium strontium titanate heterojunction;
and sixthly, putting the graphene-barium strontium titanate heterojunction into an oven for drying to obtain the high-sensitivity temperature sensor based on the graphene/barium strontium titanate heterojunction.
The chemical general formula of the Graphene/barium strontium titanate heterojunction is Graphene (Graphene)/BaxSr1- xTiO3(0.1≤x≤0.4)。
The preparation method of the high-sensitivity temperature sensor based on the graphene/barium strontium titanate heterojunction has the following beneficial effects:
the quantity of positive and negative charges adsorbed by ferroelectric dipoles in different directions in barium strontium titanate has adsorption and repulsion effects on large pi bonds in graphene. This behavior can affect the carrier mobility and resistivity of graphene. Specifically, the change of the physical state of the large pi bond has a significant influence on the charge transfer characteristics, the electric dipole disappears along with the increase of the temperature near the curie temperature of the barium strontium titanate heterostructure, and meanwhile, the positive and negative charges adsorbed on the surface of the barium strontium titanate disappear, so that the physical state of the large pi bond in the graphene changes, and further the carrier mobility of the graphene changes. Thus, when a small temperature adjustment is made around the curie temperature of barium strontium titanate, the current of the graphene/barium strontium titanate heterostructure changes significantly at a constant applied voltage.
According to the graphene/barium strontium titanate heterostructure provided by the invention, the phase transition temperature of barium strontium titanate is 0-90 ℃, the current of the heterojunction can change greatly under a certain constant voltage condition near the phase transition temperature of barium strontium titanate, when the temperature rises to be near the phase transition temperature, the current respectively rises at a higher rate than the room temperature, and the current has a very high current change rate in a narrow phase transition temperature region, so that the detection sensitivity is high.
The ceramic material prepared by the solid-phase sintering method has the advantages of simple required process and equipment, easily obtained raw materials, low cost, easy device integration, suitability for industrial production and provision of the application of the graphene/ferroelectric material heterojunction in the field of temperature sensors.
Drawings
FIG. 1 is a flow chart of the preparation of the high-sensitivity temperature sensor of graphene/barium strontium titanate heterojunction according to the present invention;
FIG. 2 shows Ba obtained in example 30.7Sr0.3TiO3The dielectric constant of (1) is along the curve chart of the change of temperature, and the frequency is 1kHz, 10kHz, 100kHz and 1MHz in sequence along the direction of an arrow;
FIG. 3 is a graph of the change of G peak of graphene with temperature;
FIG. 4 is a graph of the 2D peak of graphene as a function of temperature;
FIG. 5 shows the graphene/Ba obtained in example 3 under constant pressure0.7Sr0.3TiO3A graph of heterojunction current versus temperature;
FIG. 6 shows the graphene/Ba obtained in example 3 under constant pressure0.7Sr0.3TiO3Heterojunction resistance curve with temperature variationAnd (6) line drawing.
Detailed Description
The first embodiment is as follows: the preparation method of the high-sensitivity temperature sensor based on the graphene/barium strontium titanate heterojunction is implemented according to the following steps:
firstly, adopting a solid-phase sintering method according to BaxSr1-xTiO3Preparing barium strontium titanate ceramic according to the stoichiometric ratio and polishing;
secondly, cutting the graphene loaded on the copper sheet, and spin-coating a layer of polymethyl methacrylate on the graphene to obtain the spin-coated graphene;
thirdly, putting the spin-coated graphene into a copper etching solution, fishing out the graphene from the copper etching solution, and putting the graphene into deionized water for cleaning to obtain clean graphene;
transferring the cleaned graphene to a polished surface of the barium strontium titanate ceramic by adopting a wet transfer method, and then putting the barium strontium titanate ceramic into an oven for drying to obtain dried barium strontium titanate ceramic;
fifthly, putting the dried barium strontium titanate ceramic into acetone to dissolve polymethyl methacrylate on the surface of the graphene, and then putting the graphene into deionized water to clean the graphene and the barium strontium titanate heterojunction to obtain the graphene-barium strontium titanate heterojunction;
and sixthly, putting the graphene-barium strontium titanate heterojunction into an oven for drying to obtain the high-sensitivity temperature sensor based on the graphene/barium strontium titanate heterojunction.
The embodiment constructs a temperature sensor through graphene and ferroelectric materials, and the temperature sensor can work under different temperature conditions based on a graphene/ferroelectric heterostructure.
The second embodiment is as follows: the difference between this embodiment and the specific embodiment is that the first step is represented by the chemical formula BaxSr1- xTiO3Wherein x is not less than 0.1 and not more than 0.4.
The third concrete implementation mode: the difference between the first and second embodiments is that the solid-phase sintering method in the first step is sintering at 1200-1450 ℃ for 6-12 hours.
The fourth concrete implementation mode: the difference between this embodiment and the third embodiment is that the solid-phase sintering method in step one is sintering at 1300 ℃ for 8 hours.
The fifth concrete implementation mode: the difference between the present embodiment and one of the first to the fourth embodiments is that the copper sheet cut in the second step has a size of (4-8) × (2-5) mm.
The sixth specific implementation mode: the difference between the first embodiment and the fifth embodiment is that the graphene spin-coated in the third step is put into a copper etching solution for treatment for 10-50 minutes.
The purpose of the etching of this embodiment is to remove the graphene from the copper load so as to transfer it to the barium strontium titanate polished surface.
The seventh embodiment: the difference between the present embodiment and the first to sixth embodiments is that the graphene in the third step is put into deionized water to be washed for 5-30 minutes, and the washing is repeated for 3-5 times.
According to the embodiment, the residual etching liquid on the graphene is removed through deionized water cleaning treatment, so that the influence of the etching liquid on the heterostructure is avoided.
The specific implementation mode is eight: the difference between the first embodiment and the seventh embodiment is that the drying temperature in the fourth step is 50-80 ℃, and the drying time is 30-90 minutes.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiment is that in the fifth step, the dried barium strontium titanate ceramic is put into acetone for dissolution treatment for 5 to 30 minutes.
The barium strontium titanate ceramic dried by the embodiment can be put into acetone for repeated treatment for 3-5 times. The purpose of using acetone is to completely dissolve the polymethylmethacrylate, remove its influence on the heterostructure and simultaneously allow the electrodes to be simultaneously evaporated on the graphene and the barium strontium titanate.
The detailed implementation mode is ten: the difference between the first embodiment and the ninth embodiment is that the drying temperature in the sixth step is 50-80 ℃, and the drying time is 30-90 minutes.
The concrete implementation mode eleven: the difference between this embodiment and the first to tenth embodiments is that, in the sixth step, a gold electrode is deposited on the graphene surface of the high-sensitivity temperature sensor based on the graphene/barium strontium titanate heterojunction by using a vacuum evaporation method.
Example 1: the embodiment is based on Graphene/barium strontium titanate heterojunction (Graphene/Ba)0.9Sr0.1TiO3) The preparation method of the high-sensitivity temperature sensor is implemented according to the following steps:
according to Ba0.9Sr0.1TiO3Stoichiometric ratio of (A) weighing raw Material BaCO3，TiO2And SrCO3Sintering at 1250 ℃ for 8 hours by adopting a solid-phase sintering method to prepare Ba0.9Sr0.1TiO3Carrying out ceramic polishing;
cutting the graphene loaded on the copper sheet, and spin-coating a layer of polymethyl methacrylate on the graphene to obtain the spin-coated graphene so as to play a bearing role in transferring the graphene;
thirdly, putting the spin-coated graphene into a copper etching solution for 30 minutes, fishing the graphene from the copper etching solution by using a copper net, putting the graphene into deionized water for cleaning for 20 minutes, and removing the etching solution remained on the graphene to obtain the cleaned graphene;
transferring the cleaned graphene to a polished surface of the barium strontium titanate ceramic by adopting a wet transfer method, and then drying the barium strontium titanate ceramic in a drying oven at 60 ℃ for 60 minutes to obtain dried barium strontium titanate ceramic;
fifthly, putting the dried barium strontium titanate ceramic into acetone for 20 minutes to dissolve the polymethyl methacrylate on the surface of the graphene, repeatedly putting the acetone for 3 times to completely remove the polymethyl methacrylate, and then putting the graphene into deionized water to be cleaned up to obtain the graphene-barium strontium titanate heterojunction;
and sixthly, placing the graphene-barium strontium titanate heterojunction into an oven to be dried for 60 minutes at the temperature of 60 ℃ to obtain the high-sensitivity temperature sensor based on the graphene/barium strontium titanate heterojunction.
In this embodiment, two gold electrodes are evaporated on the surface of the graphene/barium strontium titanate heterojunction by using a vacuum evaporation method before testing.
Example 2: the embodiment is based on Graphene/barium strontium titanate heterojunction (Graphene/Ba)0.8Sr0.2TiO3) The preparation method of the high-sensitivity temperature sensor is implemented according to the following steps:
according to Ba0.8Sr0.2TiO3Stoichiometric ratio of (A) weighing raw Material BaCO3，TiO2And SrCO3Sintering at 1300 ℃ for 8 hours by adopting a solid-phase sintering method to prepare Ba0.8Sr0.2TiO3A ceramic;
cutting the graphene loaded on the copper sheet, and spin-coating a layer of polymethyl methacrylate on the graphene to obtain the spin-coated graphene so as to play a bearing role in transferring the graphene;
thirdly, putting the spin-coated graphene into a copper etching solution for 35 minutes, fishing the graphene from the copper etching solution by using a copper net, putting the graphene into deionized water for cleaning for 20 minutes, and removing the etching solution remained on the graphene to obtain the cleaned graphene;
transferring the cleaned graphene to a polished surface of the barium strontium titanate ceramic by adopting a wet transfer method, and then putting the barium strontium titanate ceramic into an oven to be dried for 50 minutes at 60 ℃ to obtain dried barium strontium titanate ceramic;
fifthly, putting the dried barium strontium titanate ceramic into acetone for 20 minutes to dissolve the polymethyl methacrylate on the surface of the graphene, repeatedly putting the acetone for 3 times to completely remove the polymethyl methacrylate, and then putting the graphene into deionized water to be cleaned up to obtain the graphene-barium strontium titanate heterojunction;
and sixthly, placing the graphene-barium strontium titanate heterojunction into an oven to be dried for 50 minutes at the temperature of 60 ℃ to obtain the high-sensitivity temperature sensor based on the graphene/barium strontium titanate heterojunction.
Example 3: this example differs from example 1 in that step one is according to Ba0.7Sr0.3TiO3Stoichiometric ratio of (A) weighing raw Material BaCO3，TiO2And SrCO3Sintering at 1350 deg.C for 10 hr by solid-phase sintering methodPrepare Ba0.7Sr0.3TiO3A ceramic.
Example 4: this example differs from example 1 in that step one is according to Ba0.6Sr0.4TiO3Stoichiometric ratio of (A) weighing raw Material BaCO3，TiO2And SrCO3Sintering at 1350 deg.C for 10 hr by solid-phase sintering method to obtain Ba0.6Sr0.4TiO3A ceramic.
Fig. 1 is a flow chart of a process for preparing a graphene/barium strontium titanate heterostructure, which corresponds to embodiments 1 to 4, and shows a process for preparing the graphene/barium strontium titanate heterostructure, in which graphene loaded on a copper sheet with a specification of (4-8) × (2-5) mm is cut, a layer of polymethyl methacrylate is spin-coated on the graphene, the spin-coated graphene is put into a copper etching solution for 10-50 minutes, after being cleaned, the cleaned graphene is transferred to a polished surface of barium strontium titanate by a wet transfer method to preliminarily form the graphene/barium strontium titanate heterostructure, after being dried, the graphene is put into acetone to completely dissolve the polymethyl methacrylate, after being cleaned and dried again, a gold electrode with a certain area is deposited by a vacuum evaporation method, and preparation is made for electrical property testing.
FIG. 2 shows Ba0.7Sr0.3TiO3The dielectric constant versus temperature curve, which corresponds to example 3, shows that the dielectric constant at different temperatures initially increases with increasing test frequency and subsequently decreases with increasing test frequency. A single dielectric peak appears around 30 c due to the transition from the ferroelectric phase to the paraelectric phase, indicating Ba0.7Sr0.3TiO3The phase transition temperature of (1), (2) and (4) is-30 ℃ (wherein the phase transition temperatures of the barium strontium titanate ceramics obtained in examples 1, 2 and 4 are-90 ℃, 60 ℃ and 0 ℃, respectively), and the barium strontium titanate ceramics are regions where electric dipoles exist and disappear before and after 30 ℃, and at the same time, the adsorbed charges disappear, so that the physical state of the large pi bond of the graphene is changed, thereby further influencing the mobility of carriers in the graphene, and macroscopically representing the change of heterojunction current and resistance.
Fig. 3 and 4 are graphs showing the change of a G peak and a 2D peak of graphene with temperature, which correspond to embodiments 1 to 4, and it can be seen from the graphs that the rule of the G peak and the 2D peak with temperature is obvious, because before the phase change of barium strontium titanate, the graphene and barium strontium titanate are in a mutual adsorption state, the lateral vibration of the graphene is affected in the current-voltage test process, after the phase change, the adsorption state of the graphene and barium strontium titanate disappears, and the lateral contraction of the graphene is not limited in the current-voltage test process, so the G peak area of the temperature-variable raman shows an increasing trend near the phase change temperature, and the temperature continues to be increased, and tends to be stable. On the other hand, before phase transition, the adsorption effect of the positive charges on the surface of barium strontium titanate on the large pi bonds of the graphene causes the longitudinal vibration of the graphene to be large, after the phase transition, the adsorption state disappears, and the longitudinal vibration is reduced, so that the 2D peak area of the temperature-variable Raman shows a reduction trend near the phase transition temperature, the temperature is continuously increased, and the temperature tends to be stable.
FIG. 5 shows graphene/Ba under constant pressure0.7Sr0.3TiO3The heterojunction current curve with temperature variation; this figure corresponds to example 3, where the current is 16.33 μ A at room temperature, and initially increases slightly with increasing temperature. The current starts to increase significantly from 16.38 μ Α to 16.99 μ Α, increasing by 0.3% and 4%, respectively, as the ambient temperature crosses the phase transition temperature of barium strontium titanate, these results indicating a higher relative change in heterostructure current around the phase transition temperature of barium strontium titanate.
FIG. 6 shows graphene/Ba under constant pressure0.7Sr0.3TiO3Heterojunction resistance versus temperature curve. The graph corresponds to example 3, and the relative change percentages of the resistance are 0.3% and 3.9% respectively at a temperature of 27-31 ℃, and the average change ratio is 0.9%/° c. However, at temperatures below the phase transition temperature, the average change ratio is only 0.06%/deg.C, and above the phase transition temperature by 0.38%/deg.C. Therefore, the resistance of the heterostructure drops to a maximum near the phase transition temperature of barium strontium titanate.
Claims (11)
1. The preparation method of the high-sensitivity temperature sensor based on the graphene/barium strontium titanate heterojunction is characterized by comprising the following steps:
firstly, adopting a solid-phase sintering method according to BaxSr1-xTiO3Preparing barium strontium titanate ceramic according to the stoichiometric ratio and polishing;
secondly, cutting the graphene loaded on the copper sheet, and spin-coating a layer of polymethyl methacrylate on the graphene to obtain the spin-coated graphene;
thirdly, putting the spin-coated graphene into a copper etching solution, fishing out the graphene from the copper etching solution, and putting the graphene into deionized water for cleaning to obtain clean graphene;
transferring the cleaned graphene to a polished surface of the barium strontium titanate ceramic by adopting a wet transfer method, and then putting the barium strontium titanate ceramic into an oven for drying to obtain dried barium strontium titanate ceramic;
fifthly, putting the dried barium strontium titanate ceramic into acetone to dissolve polymethyl methacrylate on the surface of the graphene, and then putting the graphene into deionized water to clean the graphene and the barium strontium titanate heterojunction to obtain the graphene-barium strontium titanate heterojunction;
and sixthly, putting the graphene-barium strontium titanate heterojunction into an oven for drying to obtain the high-sensitivity temperature sensor based on the graphene/barium strontium titanate heterojunction.
2. The method for preparing a high-sensitivity temperature sensor based on graphene/barium strontium titanate heterojunction according to claim 1, characterized by comprising the step of preparing a compound of formula BaxSr1-xTiO3Wherein x is not less than 0.1 and not more than 0.4.
3. The method for preparing a high-sensitivity temperature sensor based on graphene/barium strontium titanate heterojunction according to claim 1, wherein the solid-phase sintering method in the step one is sintering at 1200-1450 ℃ for 6-12 hours.
4. The method for preparing a high-sensitivity temperature sensor based on graphene/barium strontium titanate heterojunction according to claim 3, wherein the solid-phase sintering method in the step one is sintering at 1300 ℃ for 8 hours.
5. The preparation method of the graphene/barium strontium titanate heterojunction-based high-sensitivity temperature sensor according to claim 1, wherein the copper sheet cut in the second step is (4-8) x (2-5) mm in size.
6. The preparation method of the high-sensitivity temperature sensor based on the graphene/barium strontium titanate heterojunction according to claim 1, wherein the graphene subjected to spin coating in the third step is placed in a copper etching solution for treatment for 10-50 minutes.
7. The preparation method of the graphene/barium strontium titanate heterojunction-based high-sensitivity temperature sensor according to claim 1, wherein the graphene in the third step is put into deionized water to be washed for 5-30 minutes, and is repeatedly washed for 3-5 times.
8. The preparation method of the graphene/barium strontium titanate heterojunction-based high-sensitivity temperature sensor according to claim 1, wherein the drying temperature in the fourth step is 50-80 ℃ and the drying time is 30-90 minutes.
9. The preparation method of the graphene/barium strontium titanate heterojunction-based high-sensitivity temperature sensor according to claim 1, wherein in the fifth step, the dried barium strontium titanate ceramic is placed in acetone for dissolution treatment for 5-30 minutes.
10. The preparation method of the graphene/barium strontium titanate heterojunction-based high-sensitivity temperature sensor according to claim 1, wherein the drying temperature in the sixth step is 50-80 ℃ and the drying time is 30-90 minutes.
11. The preparation method of the high-sensitivity temperature sensor based on the graphene/barium strontium titanate heterojunction as claimed in claim 1, wherein in the sixth step, a gold electrode is deposited on the graphene surface of the high-sensitivity temperature sensor based on the graphene/barium strontium titanate heterojunction by a vacuum evaporation method.
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